黄瓜粉中氯吡脲残留分析标准物质研究

Development of Certified Reference Material for Forchlorfenuron Residue in Cucumber Powder

基体标准物质(CRMs)在验证分析方法和质量控制中起着重要作用。为保证植物生长调节剂风险评估结果的准确性和可靠性,首次研制了黄瓜粉中氯吡脲标准物质,以提高黄瓜中氯吡脲残留测量质量。实验经制浆、加药、均质、冷冻干燥、研磨、筛分、混合、包封等工序制备了标准物质候选物;优化并建立了液相色谱-串联同位素稀释质谱法(ID-LC/MS/MS)定值方法,并将其用于标准物质的定值。结果表明,黄瓜粉中氯吡脲特性量值为14.7 mg/kg,扩展不确定度为2.7 mg/kg(k=2)。同时,还评估了特性量的均匀性,以及在-20℃下9个月的长期稳定性和40℃条件下9天的短期稳定性,并全面分析与评估了定值、均匀性和稳定性的引入的不确定度。

Matrix certified reference materials(CRMs)play a crucial role in validating analytical methods and ensuring quality control.To enhance the accuracy and reliability of risk assessments for plant growth regulators,we have developed a certified reference material(CRM)for forchlorfenuron in cucumber powder,thereby improving the measurement quality of forchlorfenuron residues in cucumbers.The CRM was prepared through processes including pulping,drug-adding,homogenization,freeze-drying,grinding,sieving,mixing,and encapsulation.The liquid chromatography-tandem isotope dilution mass spectrometry(ID-LC/MS/MS)method was optimized and established for the quantification of the CRM.The certified value of forchlorfenuron in cucumber powder was determined to be 14.7 mg/kg with an expanded uncertainty of 2.7 mg/kg(k=2).Furthermore,the homogeneity of the material was assessed,along with its long-term stability at−20°C over nine months and short-term stability at 40°C over nine days.The study comprehensively evaluated uncertainties introduced by characterization,homogeneity,and stability assessments.